CN109504339A - Hydroxyl polysiloxane end blocking method and transparent two-component are condensed room temperature vulcanization silica gel - Google Patents
Hydroxyl polysiloxane end blocking method and transparent two-component are condensed room temperature vulcanization silica gel Download PDFInfo
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- CN109504339A CN109504339A CN201811434774.XA CN201811434774A CN109504339A CN 109504339 A CN109504339 A CN 109504339A CN 201811434774 A CN201811434774 A CN 201811434774A CN 109504339 A CN109504339 A CN 109504339A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a kind of hydroxyl polysiloxane end blocking methods and transparent two-component to be condensed room temperature vulcanization silica gel, and end blocking method is: at 150 DEG C of temperature, vacuum degree 0.08MPa, dehydrating hydroxyl polysiloxane 4 hours, cooling discharging；By weight, it is added in the reaction vessel through 100 parts of dewatered hydroxyl polysiloxane, under nitrogen protection, 0.5~2.5 part of end-capping reagent, 0.01~0.02 part of NaOH catalyst is added, kept for 25 DEG C of temperature stir 1 hour；Upper step solution is neutralized to PH=7 with 0.2 part of HCl, is evaporated under reduced pressure and takes off the alcohols that low removal reaction generates, obtain alkoxy end-capped hydroxyl polysiloxane.The silica gel of preparation are as follows: by weight, component A: 0.0005~0.002 part of 100 parts of hydroxyl polysiloxane, the organotin catalysts containing above-mentioned sealing end；B component: 10 parts of 50~75 parts of hydroxyl polysiloxane, ethyl orthosilicate after 15~40 parts of hydroxy resin, dehydration.The present invention assigns silica gel certain transparency and intensity, and can realize component A:B=1:1.
Description
Technical field
The present invention relates to two-components to be condensed room curing silicon rubber field, especially a kind of hydroxyl polysiloxane end blocking method
And a kind of transparent two-component is condensed room temperature vulcanization silica gel.
Background technique
LED industry development is just being sent out towards directions such as more high brightness, more high weather resistance and higher production efficiencys at present
Exhibition.The presently used encapsulating material of LED has the high transparent material such as epoxy resin, polymethyl methacrylate, glass, organosilicon,
Middle epoxy resin and organosilicon material are as main encapsulating material, and epoxy resin internal stress is excessive, xanthochromia, high and low temperature resistance
Difference, loss of properties on aging, and current organosilicon material, internal stress are small, high and low temperature resistance is good, non yellowing.
LED flexible light bar has as a kind of LED illumination device to be widely applied, it uses FPC (flexible circuitry soft board)
Assembling wiring board is done, is assembled with paster LED.FPC material is soft, can arbitrarily be bent, folds, wind, can be in three-dimensional space
Between arbitrarily move and flexible without fractureing, be suitable for the various patterns of any combination in ad decoration；It can also arbitrarily cut,
Can also arbitrarily extend and shine unaffected, luminescent color is changeable, tunable optical, controllable colour variation, may be selected it is monochromatic and
The effect of RGB, energy band give environment colorful in riotous profusion visual effect, are widely used to furniture, automobile, advertisement, showcase, wheel at present
The fields such as ship and landscape light in city.
Traditional condensed type casting glue carries out mechanics reinforcement generally by white carbon black, such material after reinforcement is mixed
Turbid translucent product, although and additional organosilicon casting glue can carry out reinforcement by MQ resin to guarantee that its is good
Lightness, but such product is significantly worse than condensed type casting glue in terms of cementability and bonding substrate adaptability.
Two-component condensation room temperature curing silica gel can be used for encapsulating or surface coating, currently marketed this kind of product or guarantee
Transparency but without intensity, or have some strength but transparency is very poor, and it had not only been able to satisfy intensity requirement, but also there is 100% light transmission
The opaque products of rate are rarely found in the market, in addition, two components of A, B of commercially available conventional two-component condensation room temperature curing silica gel
Ratio be mostly 10:1 or 100:2~3, disadvantage is that: two component weight ratio differences are bigger, so existing mixed
Conjunction is uniformly relatively difficult to achieve, and when especially matching glue using machine, it is even more impossible to matching units, influence production efficiency.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of hydroxyl polysiloxane end blocking methods and transparent two-component to contract
Room temperature vulcanization silica gel is closed, using hydroxy resin reinforcement, assigns product certain transparency and intensity, by hydroxyl polysiloxane (107
Glue) it is dehydrated and is blocked operation, the activity of base rubber is reduced, realizes the use ratio of component A:B=1:1.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of hydroxyl polysiloxane end blocking method, comprising the following steps:
Step 1: under conditions of 150 DEG C of temperature, vacuum degree 0.08MPa, dehydrate hydroxyl polysiloxane 4 hours, it
Cooling discharging afterwards；
Step 2: by weight, be added in the reaction vessel through 100 parts of dewatered hydroxyl polysiloxane, in nitrogen protection
Under, 0.5~2.5 part of end-capping reagent, 0.01~0.02 part of NaOH catalyst is added, is kept for 25 DEG C of temperature stir 1 hour；
Step 3: step 2 solution being neutralized to PH=7 with 0.2 part of HCl, is evaporated under reduced pressure and takes off the alcohol that low removal reaction generates
Class obtains alkoxy end-capped hydroxyl polysiloxane.
Further, in step 1, it is dehydrated using kneader.
Further, in step 2, the end-capping reagent is three second of ethyl orthosilicate, methyltrimethoxysilane or methyl
Oxysilane.
Further, 1 part of the end-capping reagent, the NaOH catalyst are 0.016 part.
A kind of transparent two-component condensation room temperature vulcanization silica gel, contains the hydroxyl polysiloxane prepared using the above method,
Specifically: by weight, component A: 0.0005~0.002 part of 100 parts of hydroxyl polysiloxane, the organotin catalysts of sealing end；B group
Point: 10 parts of 50~75 parts of hydroxyl polysiloxane, ethyl orthosilicate after 15~40 parts of hydroxy resin, dehydration.
Further, the organotin catalysts are dibutyl tin dilaurate.
Further, the organotin catalysts are 0.001 part, and the hydroxy resin is 30 parts, after the dehydration
Hydroxyl polysiloxane be 60 parts.
Compared with prior art, the beneficial effects of the present invention are:
1) hydroxy resin reinforcement is used, assigns product certain transparency and intensity, so that product is fully transparent after solidification,
Tensile strength is 1.3~2.5MPa (intensity of commercial clear class product is generally 0.2~0.6MPa).
2) hydroxyl polysiloxane is dehydrated and is blocked operation, reduce the activity of base rubber, to realize component A:B=
The use ratio of 1:1 improves service efficiency so that machine industrialization is achieved.
Detailed description of the invention
Fig. 1 is hydroxyl polysiloxane end blocking method flow chart in the present invention.
Fig. 2 is that transparent two-component condensation room temperature vulcanization silica gel component A matches drawing in the present invention.
Fig. 3 is that transparent two-component condensation room temperature vulcanization silica gel B component matches drawing in the present invention.
Specific embodiment
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Embodiment 1
A kind of hydroxyl polysiloxane end blocking method, comprising the following steps:
Step 1: under conditions of 150 DEG C of temperature, vacuum degree 0.08MPa, it is (viscous that kneader dehydrates hydroxyl polysiloxane
Degree is 20,000 cs) 4 hours, later cooling discharging；
Step 2: by weight, it is added in flask through 100 parts of dewatered hydroxyl polysiloxane, under nitrogen protection,
1 part of ethyl orthosilicate, 0.016 part of NaOH catalyst is added, is kept for 25 DEG C of temperature stir 1 hour；
Step 3: step 2 solution being neutralized to PH=7 with 0.2 part of HCl, is evaporated under reduced pressure and takes off the alcohol that low removal reaction generates
Class obtains alkoxy end-capped hydroxyl polysiloxane.
Transparent two-component condensation room temperature vulcanization silica gel is prepared according to the hydroxyl polysiloxane obtained by the above method blocked,
Specifically: by weight, component A: 100 parts of hydroxyl polysiloxane, the dibutyl tin dilaurate 0.0005~0.002 of sealing end
Part；B component: 70 parts of hydroxyl polysiloxane (viscosity 5000cs) after 20 parts of end group resin (10,000 cs of viscosity), dehydration, just
10 parts of silester.
The transparent two-component condensation room temperature vulcanization silica gel quality index of gained is: before solidification: 20,000 cs of component A viscosity, B component
Viscosity 7000cs, after solidification, anti-Qiang Qiangdu: 1.8Mpa, elongation: 130%, light transmittance: 100%.
Embodiment 2
A kind of hydroxyl polysiloxane end blocking method, comprising the following steps:
Step 1: under conditions of 150 DEG C of temperature, vacuum degree 0.08MPa, it is (viscous that kneader dehydrates hydroxyl polysiloxane
Degree is 50,000 cs) 4 hours, later cooling discharging；
Step 2: by weight, be added in the reaction vessel through 100 parts of dewatered hydroxyl polysiloxane, in nitrogen protection
Under, 0.5 part of methyltrimethoxysilane, 0.01 part of NaOH catalyst is added, is kept for 25 DEG C of temperature stir 1 hour；
Step 3: step 2 solution being neutralized to PH=7 with 0.2 part of HCl, is evaporated under reduced pressure and takes off the alcohol that low removal reaction generates
Class obtains alkoxy end-capped hydroxyl polysiloxane.
Transparent two-component condensation room temperature vulcanization silica gel is prepared according to the hydroxyl polysiloxane obtained by the above method blocked,
Specifically: by weight, component A: 100 parts of hydroxyl polysiloxane, the dibutyl tin dilaurate 0.0005~0.002 of sealing end
Part；B component: 60 parts of hydroxyl polysiloxane (20,000 cs of viscosity), positive silicon after 30 parts of hydroxy resin (20,000 cs of viscosity), dehydration
10 parts of acetoacetic ester.
The transparent two-component condensation room temperature vulcanization silica gel quality index of gained is: before solidification: 50,000 cs of component A viscosity, B component
20,000 cs of viscosity, after solidification, anti-Qiang Qiangdu: 2.5Mpa, elongation: 250%, light transmittance: 100%.
Embodiment 3
A kind of hydroxyl polysiloxane end blocking method, comprising the following steps:
Step 1: under conditions of 150 DEG C of temperature, vacuum degree 0.08MPa, (viscosity is dehydration and drying hydroxyl polysiloxane
3000cs) 4 hours, cooling discharging later；
Step 2: by weight, be added in the reaction vessel through 100 parts of dewatered hydroxyl polysiloxane, in nitrogen protection
Under, 2.5 parts of methyltriethoxysilane, 0.02 part of NaOH catalyst are added, are kept for 25 DEG C of temperature stir 1 hour；
Step 3: step 2 solution being neutralized to PH=7 with 0.2 part of HCl, is evaporated under reduced pressure and takes off the alcohol that low removal reaction generates
Class obtains alkoxy end-capped hydroxyl polysiloxane.
Transparent two-component condensation room temperature vulcanization silica gel is prepared according to the hydroxyl polysiloxane obtained by the above method blocked,
Specifically: by weight, component A: 100 parts of hydroxyl polysiloxane, the dibutyl tin dilaurate 0.0005~0.002 of sealing end
Part；B component: 60 parts of hydroxyl polysiloxane (viscosity 3000cs) after 30 parts of hydroxy resin (viscosity 8000cs), dehydration, just
10 parts of silester.
The transparent two-component condensation room temperature vulcanization silica gel quality index of gained is: before solidification: component A viscosity 3000cs, B component
Viscosity 5000cs, after solidification, anti-Qiang Qiangdu: 1.3Mpa, elongation: 100%, light transmittance: 100%.
Embodiment 4
A kind of hydroxyl polysiloxane end blocking method, comprising the following steps:
Step 1: under conditions of 150 DEG C of temperature, vacuum degree 0.08MPa, dehydrating hydroxyl polysiloxane (10,000 cs) 4
Hour, cooling discharging later；
Step 2: by weight, be added in the reaction vessel through 100 parts of dewatered hydroxyl polysiloxane, in nitrogen protection
Under, 2 parts of methyltrimethoxysilane, 0.01 part of NaOH catalyst are added, are kept for 25 DEG C of temperature stir 1 hour；
Step 3: step 2 solution being neutralized to PH=7 with 0.2 part of HCl, is evaporated under reduced pressure and takes off the alcohol that low removal reaction generates
Class obtains alkoxy end-capped hydroxyl polysiloxane.
Transparent two-component condensation room temperature vulcanization silica gel is prepared according to the hydroxyl polysiloxane obtained by the above method blocked,
Specifically: by weight, component A: 100 parts of hydroxyl polysiloxane, the dibutyl tin dilaurate 0.0005~0.002 of sealing end
Part；B component: 70 parts of hydroxyl polysiloxane (viscosity 5000cs) after 15 parts of hydroxy resin (10,000 cs of viscosity), dehydration, just
10 parts of silester.
The transparent two-component condensation room temperature vulcanization silica gel quality index of gained is: before solidification: 10,000 cs of component A viscosity, B component
Viscosity 6000cs, after solidification, anti-Qiang Qiangdu: 1.5Mpa, elongation: 120%, light transmittance: 100%.
In addition, when in use, can different viscosities of hydroxyl polysiloxane end blocking method preparation according to the present invention sealing end
Hydroxyl polysiloxane mix and match afterwards to meet different viscosity requirements, and then can prepare the transparent two-component of different viscosities
It is condensed room temperature vulcanization silica gel.
Since the formula of the catalytic amount of conventional two-component condensation room temperature vulcanization silica gel, cross-linked dosage and amount of resin is former
Cause can not split into 1:1 in normal ratio because certain components can not coexist, only content it is bigger 107
It is possible to split into this ratio after glue sealing end passivation.The present invention be solve existing condensed type double-component room temperature glue transparency and
The contradiction that intensity cannot be realized simultaneously realizes the proportion requirement of stable component A:B=1:1, meets machinery equipment (especially
Spraying process) requirement to glue.
In the present invention, the sealing end of 1,107 glue can select different viscosity according to the requirement of application aspect, also can choose not
Same end-capping reagent is with obtained different viscosities and the hydroxyl polysiloxane of different functional groups sealing end, to meet different casting glue difference works
The hydroxy-terminated polysiloxane that sealing end product viscosity can be 1000~50,000 such as may be selected in requirement of the skill to viscosity.2, according to product
The hydroxy resin content that intensity requirement uses is configured to the product of 1:1 ratio finally for 15%~40%, is configured to this ratio
The advantage of product is: for the product of common on the market 10:1 and 4:1, more conducively two components of A, B are uniformly mixed,
And it is more suitable for robotic production.3, the tensile strength that the product being configured to has is 1.3~2.5MPa, and product is fully transparent,
Mixing viscosity is that 1000~50,000 cs are adjustable.Hydroxy resin reinforcement hydroxy-terminated polysiloxane realizes intensity requirement, the poly- silicon of terminal hydroxy group
The dehydration of oxygen alkane and termination process are reduced activity and made with that can not be chemically reacted with longer-term after catalyst-organotin mixing,
Increase storage stability, to realize the mixed proportion of component A:B=1:1.
Claims (7)
1. a kind of hydroxyl polysiloxane end blocking method, which comprises the following steps:
Step 1: under conditions of 150 DEG C of temperature, vacuum degree 0.08MPa, dehydrating hydroxyl polysiloxane 4 hours, Zhi Houleng
But it discharges；
Step 2: by weight, it is added in the reaction vessel through 100 parts of dewatered hydroxyl polysiloxane, under nitrogen protection,
0.5~2.5 part of end-capping reagent, 0.01~0.02 part of NaOH catalyst is added, is kept for 25 DEG C of temperature stir 1 hour；
Step 3: step 2 solution being neutralized to PH=7 with 0.2 part of HCl, is evaporated under reduced pressure and takes off the alcohols that low removal reaction generates, obtain
To alkoxy end-capped hydroxyl polysiloxane.
2. a kind of hydroxyl polysiloxane end blocking method as described in claim 1, which is characterized in that in step 1, using kneading
Machine is dehydrated.
3. a kind of hydroxyl polysiloxane end blocking method as described in claim 1, which is characterized in that in step 2, the sealing end
Agent is ethyl orthosilicate, methyltrimethoxysilane or methyltriethoxysilane.
4. a kind of hydroxyl polysiloxane end blocking method as described in claim 1, which is characterized in that 1 part of the end-capping reagent, it is described
NaOH catalyst is 0.016 part.
5. a kind of transparent two-component is condensed room temperature vulcanization silica gel, which is characterized in that contain method as described in claim 1 preparation
Hydroxyl polysiloxane, specifically: by weight, component A: 100 parts of hydroxyl polysiloxane, the organotin catalysts 0.0005 of sealing end
~0.002 part；B component: 50~75 parts of hydroxyl polysiloxane, ethyl orthosilicate after 15~40 parts of hydroxy resin, dehydration
10 parts.
6. transparent two-component as claimed in claim 5 is condensed room temperature vulcanization silica gel, which is characterized in that the organotin catalysts
For dibutyl tin dilaurate.
7. transparent two-component as claimed in claim 5 is condensed room temperature vulcanization silica gel, which is characterized in that the organotin catalysts
It is 0.001 part, the hydroxy resin is 30 parts, and the hydroxyl polysiloxane after the dehydration is 60 parts.
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| CN201811434774.XA CN109504339A (en) | 2018-11-28 | 2018-11-28 | Hydroxyl polysiloxane end blocking method and transparent two-component are condensed room temperature vulcanization silica gel |
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| CN201811434774.XA CN109504339A (en) | 2018-11-28 | 2018-11-28 | Hydroxyl polysiloxane end blocking method and transparent two-component are condensed room temperature vulcanization silica gel |
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Cited By (3)
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| CN110066637A (en) * | 2019-04-02 | 2019-07-30 | 深圳市鑫业新光电有限公司 | A kind of formula and preparation method thereof of LED light backboard glue |
| CN111320964A (en) * | 2020-03-20 | 2020-06-23 | 佛山市金云信硅材料制品有限公司 | Silicone sealant and preparation method thereof |
| CN113980639A (en) * | 2021-11-02 | 2022-01-28 | 绵阳惠利电子材料有限公司 | Transparent and flowing packaging material capable of being rapidly cured at room temperature and preparation method thereof |
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Cited By (3)
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| CN110066637A (en) * | 2019-04-02 | 2019-07-30 | 深圳市鑫业新光电有限公司 | A kind of formula and preparation method thereof of LED light backboard glue |
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| CN113980639A (en) * | 2021-11-02 | 2022-01-28 | 绵阳惠利电子材料有限公司 | Transparent and flowing packaging material capable of being rapidly cured at room temperature and preparation method thereof |
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